CN104160490B - silver particles sintered body - Google Patents

silver particles sintered body Download PDF

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Publication number
CN104160490B
CN104160490B CN201380012394.6A CN201380012394A CN104160490B CN 104160490 B CN104160490 B CN 104160490B CN 201380012394 A CN201380012394 A CN 201380012394A CN 104160490 B CN104160490 B CN 104160490B
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China
Prior art keywords
silver particles
sintered body
silver
particles sintered
semiconductor device
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CN201380012394.6A
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CN104160490A (en
Inventor
小林诚
佐佐木幸司
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Nameishi Co Ltd
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Nameishi Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/3006—Ag as the principal constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
    • B23K1/0016—Brazing of electronic components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/365—Selection of non-metallic compositions of coating materials either alone or conjoint with selection of soldering or welding materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/06—Alloys based on silver
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Abstract

The silver particles sintered body of the present invention is for engaging the engagement member of the component of semiconductor device silver particles sintered body, and the creep activity energy of silver particles sintered body is 0.4~0.75 times of the lattice diffusion activation energy of block silver.

Description

Silver particles sintered body
Technical field
It, can be as engaging the engagement structure of the component of semiconductor device the present invention relates to when manufacturing semiconductor device The silver particles sintered body and its manufacturing method that part uses.The present invention is more particularly directed to can be used as convex block and die bonding material (die The silver particles sintered body and its manufacturing method of engagement members such as attach).
Background technology
Along with the miniaturization, lightweight, high performance of electronic equipment, the calorific value increase of semiconductor device and heat density Rise.In addition, in flip-chip semiconductor, occur the broken of stress zone with the low-k of interlayer dielectric The problem of damage.In addition, as power semiconductor, the big semiconductor of silicon carbide, band gap as gallium nitride is being studied.Use band The power semiconductor of the big semiconductor of gap can work at high temperature compared with previous silicon semiconductor.
As the conductive bonding material of the semiconductor device suitable for working at high temperature, for example, in patent document 1 Record following conductive bonding material, which is characterized in that have metal particle and coating metal resin particle as aggregate, it is described Metal particle includes the 1st metal and the metal particle that can be sintered at a temperature of less than the fusing point of the 1st metal, the gold It is to be coated with to burn with above-mentioned 1st metal on the particle of the resin bigger than above-mentioned metal particle grain size to belong to coated with resin particle The coating metal resin particle of 2nd metal of knot.
As the semiconductor device and its manufacturing method of flip chip type, for example, recording in patent document 2 following The manufacturing method of the semiconductor device of flip chip type, including implementing following process successively：Organic material base will be set to The process that the salient pole of electrode portion and semiconductor element on plate is electrically connected and the semiconductor element is configured on the substrate；It is right The process that the substrate surface carries out plasma treatment；And bottom as defined in the gap filling between the substrate and semiconductor element After portion's filler, defined bottom filling is made to be heating and curing, so as to the process of closing gap.
In addition, the manufacturing method of the convex block as semiconductor device, for example, Patent Document 3 discloses following electricity The manufacturing method of road connection convex block, which is characterized in that partly lead defined metal member adhesive in dotted be coated on The circuit connecting electrode portion in circuit connecting pad portion or substrate on volume elements part, 70 DEG C or more and less than 400 DEG C into The metallic, is thus sintered by row heating each other, and made of metal convex block is formed on semiconductor element or on substrate.In addition, Record the following contents in patent document 3, it is specified that metal member with adhesive be comprising (A) average grain diameter (median D50) more than 0.1 μm and less than 50 μm, fusing point higher than 400 DEG C the metallic of heat-agglomerating and (B) liquid fluxing agent Paste, by being heated in 70 DEG C or more and less than 400 DEG C, become metallic (A) and be sintered and have and gold each other Belong to the equal fusing point of particle (A) and there is the porous sintering of cementability in sintering process to the metal member of contact Object.
In addition, in patent document 4, as the convex block of semiconductor device, record by carbon nanotube (CNT) and selectivity Ground is coated the carbon nanotube projection cube structure body that the coating metal portion of the one end of the carbon nanotube is formed.In addition, in patent text The following contents is recorded in offering 4, as electrode broken string, stress zone caused by the high current density that semiconductor chip is inhibited to be possessed The damaged method come, it is proposed that the method for salient pole application carbon nanotube (CNT).
Described in patent document 5 once the average grain diameter of particle be 40~350nm, crystallite grain size be 20~70nm and Average grain diameter is relative to the silver particles that the ratio between crystallite grain size is 1~5.Invention described in patent document 5 describes its subject and exists In the raw material silver particles for providing the conductive paste that sufficient electric conductivity is shown under the firing temperature below 200 DEG C and contain this The conductive paste of silver particles.Specifically record the following contents, the conductive paste containing silver particles described in patent document 5 Can be used in the circuitous pattern of more miniaturization into.
Patent document 1：Japanese Unexamined Patent Publication 2011-238779 bulletins
Patent document 2：Japanese Unexamined Patent Publication 2010-192525 bulletins
Patent document 3：Japanese Unexamined Patent Publication 2010-131669 bulletins
Patent document 4：Japanese Unexamined Patent Publication 2008-210954 bulletins
Patent document 5：Japanese Unexamined Patent Publication 2006-183072 bulletins
Invention content
Semiconductor device has semiconductor element (semiconductor chip) with being used to place the lead frame of semiconductor element and match The structure that line substrate etc. is connected across grafting materials such as die bonding material, convex blocks.In addition, semiconductor device also has two sometimes The structure that a above semiconductor element, silicon intermediary layer are connected with each other across grafting material.The semiconductor device of the structure is being applied Added temperature cycles when heat supply when, due to the difference of supporting mass and the coefficient of thermal expansion of semiconductor element connecting portion generate should Power.Therefore, semiconductor element is appeared in, the interface of crackle or grafting material and semiconductor element or supporting mass occurs for grafting material The problem of peeling-off.
It is therefore desirable to be able to reduce the connecting material of the stress of connecting portion.
In addition, in order to the high speed of the rising of the Reflow Soldering temperature without Pbization of solder, semiconductor work, as layer Between insulating film always using weak low-k (Low-K) material of mechanical strength.In addition, it with the high speed of semiconductor, puts Hot, convex block narrow pitch turns to purpose, always using the convex block of Cu rod structures.The stress that semiconductor device applies is become as a result, Greatly.Therefore, it is necessary to be used to prevent the more high-tech of semiconductor device breakage.
In addition, other than the raising of the highly integrated and operating rate of semiconductor device, in the field of power semiconductor In also in the research for carrying out the high semiconductor of operating temperature.Thus, it is desirable to conductivity and the heat conductivity connection material higher than solder Material.
In addition, as high thermal conductivity die bonding material, the material of convex block, usually using kupper solder etc..But due to lead Harmfulness, the lead of various countries use system limit it is more stringent.Therefore, the high fever for being required to the replacement as kupper solder in recent years passes The property led die bonding material.
It records in patent document 1 and has metal particle and be coated on the grain size resin particle bigger than metal particle golden Conductive bonding material of the coating metal resin particle of category as aggregate.But using such coating metal resin During particle, there are problems that low stress is in the relationship of tradeoff with conductivity, thermal conductivity and is difficult to take into account.
It records in patent document 4 and is used using carbon nanotube (CNT) as the convex block of semiconductor device.But due to The manufacturing process of carbon nanotube is complicated, therefore is difficult to obtain high production rate.
Therefore, it is an object of the invention to obtain to mitigate the stress of semiconductor device and it is conductive, for connecing Close the engagement member of the component of semiconductor device.In particular it is object of the present invention to obtain following engagement member, this connects Closing component can be produced by mitigating the difference due to the coefficient of thermal expansion of the semiconductor chip and supporting mass of IC, MOSFET, LED etc. Raw strain, so as to inhibit crackle of semiconductor device generation etc..In addition, it is an object of the invention to obtain can be used as replacing lead The engagement member of the high thermal conductivity die bonding material of solder.In addition, it is an object of the invention to obtain can efficiency well The very excellent engagement member of heat, exothermic character that diffusion is generated by semiconductor element.
The present inventor effort with great concentration as a result, it has been found that, silver particles sintered body of the invention is it is surprising that show Special creep behaviour in a low temperature of in the past unknown.The present inventor is in view of the discovery is further verified repeatedly.As a result, this Inventor has found, if the silver particles sintered body for the present invention for showing special creep behaviour to be used as to the engagement structure of semiconductor device Part can then mitigate the stress of semiconductor device, so that completing the present invention.That is, in order to solve the above problems, the present invention have with Under technical solution.
(technical solution 1)
The present invention relates to a kind of silver particles sintered bodies, are for engaging the engagement member of the component of semiconductor device silver Microparticles sinter body, wherein, the creep activity energy of silver particles sintered body is the 0.4~0.75 of the lattice diffusion activation energy of block silver Times.In accordance with the invention it is possible to obtain to mitigate the stress of semiconductor device and it is conductive, for engage semiconductor dress The engagement member for the component put.
(technical solution 2)
The creep activity energy of the preferred silver particles sintered body of silver particles sintered body of the present invention is that the lattice diffusion of block silver is lived Change energy 0.4~0.7 times.By making the creep activity energy of silver particles sintered body 0.4 for the lattice diffusion activation energy of block silver ~0.7 times, it can effectively mitigate the stress of semiconductor device.
(technical solution 3)
The silver particles sintered body of the present invention is 40~350nm, micromeritics preferably by by the average grain diameter of primary particle Diameter is 20~70nm and the ratio between average grain diameter and crystallite grain size are heated to 130~320 DEG C of temperature and are sintered for 1~5 silver particles Silver particles sintered body.By being burnt into defined silver particles, i.e., it is sintered, can be cut by being heated to set point of temperature The silver particles sintered body with advantageous feature of the present invention is obtained on the spot.
(technical solution 4)
For the silver particles sintered body of the present invention, the gap of silver particles sintered body can be filled by resin.The present invention Silver particles sintered body contain resin in the gap of silver particles sintered body in the case of, also can show very high electric conductivity simultaneously Show special creep behaviour.
(technical solution 5)
The present invention relates to the semiconductor devices that a kind of semiconductor chip is engaged with supporting mass by engagement member, are engagement structures Part is the semiconductor device of above-mentioned silver particles sintered body.If the silver particles sintered body of the present invention is used as by semiconductor chip The engagement member engaged with supporting mass, then since exothermic character is very excellent, can efficiency spread well by semiconductor The heat that element generates.
(technical solution 6)
It is partly led via what convex block engaged with wiring substrate or the second semiconductor chip the present invention relates to the first semiconductor chip Body device, be convex block part or all be above-mentioned silver particles sintered body semiconductor device.If the silver by the present invention is micro- Grain sintered body is used as convex block, then can by mitigate the difference due to the coefficient of thermal expansion of the chip and substrate of MOSFET, LED etc. and The strain of generation, so as to inhibit crackle generated in semiconductor device etc..
(technical solution 7)
The present invention relates to a kind of manufacturing methods of silver particles sintered body, are for engaging connecing for the component of semiconductor device The manufacturing method of component silver particles sintered body is closed, including by being 40~350nm, crystallite by the average grain diameter of primary particle The silver particles that grain size is 20~70nm and the ratio between average grain diameter and crystallite grain size are 1~5 be heated to 130~320 DEG C of temperature come into The process of row sintering.Using the manufacturing method of the present invention, it can obtain mitigating the stress of semiconductor device and conductive , engagement member for engaging the component of semiconductor device.
(forming 8)
The present invention relates to a kind of manufacturing methods of semiconductor device, are that semiconductor chip is connect with supporting mass by engagement member The manufacturing method of the semiconductor device of conjunction, including following process：It is 40~350nm by the average grain diameter comprising primary particle, micro- Conductive paste including the silver particles that crystal size is 20~70nm and the ratio between average grain diameter and crystallite grain size are 1~5 is supplied to branch Hold the process on body；By the process of semiconductor chip alignment position mounting on supporting mass；With by by supporting mass, conductive paste The process for being heated to 130~320 DEG C of temperature with semiconductor chip to be sintered.If the system of the semiconductor device using the present invention Method is made, then can mitigate the stress of the engagement on supporting mass between semiconductor chip, therefore semiconductor device can be inhibited Crackle of middle generation etc..
(forming 9)
The present invention relates to a kind of manufacturing methods of semiconductor device, are the manufacturers of the semiconductor device with convex block Method, including following process：It is 40~350nm by the average grain diameter comprising primary particle, crystallite grain size is 20~70nm and average The ratio between grain size and crystallite grain size are that the conductive paste including 1~5 silver particles is supplied to the process of semiconductor chip；With pass through by The process that semiconductor chip is heated to 130~320 DEG C of temperature to be sintered.If the manufacture of the semiconductor device using the present invention Method, then can mitigate the stress of the engagement on supporting mass between semiconductor chip, therefore can inhibit in semiconductor device Crackle of generation etc..
In accordance with the invention it is possible to obtain to mitigate the stress of semiconductor device and it is conductive, for engage partly lead The engagement member of the component of body device.Specifically, following engagement member can be obtained according to the present invention, the engagement member energy Enough strains generated by mitigating the difference due to the coefficient of thermal expansion of the chip and substrate of MOSFET, LED etc., so as to inhibit half Crackle generated in conductor device etc..In addition, it in accordance with the invention it is possible to obtains can be used as the high thermal conductivity core instead of kupper solder Piece is bonded the engagement member of material.
In addition, according to the present invention it is possible to obtain can efficiency to spread the heat generated by semiconductor element, heat release well special The very excellent engagement member of property.The engagement member of the present invention has very high lead using silver as material, therefore compared with solder Heating rate.The engagement member of the present invention can efficiency spread the heat generated by semiconductor element well, therefore there is exothermic character The advantages of very excellent.
The engagement member of the semiconductor device of the present invention with high electric conductivity and heat conductivity is in semiconductor device During manufacture, high production rate and economy disclosure satisfy that.
Description of the drawings
Fig. 1 is that trus stress σ (longitudinal axis, the MPa)-true strain ε (horizontal axis, %) for the silver particles sintered body for representing embodiment 1 is bent The figure of line.
Fig. 2 is that the stress for the silver particles sintered body for representing embodiment 1 mitigates the figure of result of the test, is for horizontal stroke with the time (second) Axis, with the figure that trus stress σ (MPa) is the longitudinal axis.
Fig. 3 be the silver particles sintered body for representing embodiment 1 steady state creep speed (longitudinal axis ,/second) and stress σ (horizontal axis, MPa the figure of relationship).
Fig. 4 is the figure that Arrhenius curves are shown for the steady state creep speed and the relationship of stress shown in Fig. 3.
Fig. 5 is the schematic diagram of the mechanical test plate shape of silver particles sintered body.
Fig. 6 is the internal structure that the silver particles sintered body of the present invention is represented by 2 charge patterns of scanning electron microscope Figure.
Fig. 7 is the schematic diagram for the FEM model for representing silver particles sintered body.
Fig. 8 is that trus stress σ (longitudinal axis, the MPa)-true strain ε (horizontal axis, %) for the silver particles sintered body for representing embodiment 1 is bent The figure of line is the figure for the result for representing experiment value (experiment, solid line) and Finite Element parsing (FEM).
Fig. 9 is that the stress for the silver particles sintered body for representing embodiment 1 mitigates the figure of result of the test, is for horizontal stroke with the time (second) Axis is to represent experiment value (experiment, solid line) and the knot of Finite Element parsing (FEM) with the figure that trus stress σ (MPa) is the longitudinal axis The figure of fruit.
Figure 10 be the silver particles sintered body for representing embodiment 1 steady state creep speed (longitudinal axis ,/second) and stress σ (horizontal axis, MPa the figure of relationship).
Figure 11 is the silver particles sintered body for representing embodiment 1 and the sintering of the silver particles comprising curable resin of embodiment 4 The stress of body mitigates the figure of result of the test, is for horizontal axis, with the figure that trus stress σ (MPa) is the longitudinal axis with the time (second).
Specific embodiment
The present invention relates to a kind of silver particles sintered bodies, are for engaging the component of semiconductor device (semiconductor element (half Conductor chip) and supporting mass etc.) engagement member silver particles sintered body, the creep activity energy of silver particles sintered body is block silver 0.4~0.75 times of lattice diffusion activation energy.The inventors discovered that the silver of the present invention of creep behaviour as defined in display is micro- Grain sintered body.If it was found that the silver particles sintered body of the present invention is used as engagement member, can obtain that semiconductor device can be mitigated Stress and conductive engagement member.Hereinafter, the present invention will be described.
First, the creep behaviour of the silver particles sintered body of the present invention is illustrated.The result of the present inventor's effort with great concentration Be find the present invention silver particles sintered body show it is previous it is unknown in a low temperature of special creep behaviour (time interdependent type Deformational behavior).
The creep start temperature (absolute temperature) of common metal material be fusing point 40% (in this specification, with The form of " 0.4TM " represents.) left and right.Such as in the case of silver, fusing point 1235K, therefore 0.4TM is 494K (221 DEG C).With This is opposite, and the creep start temperature of practical block silver is 479K (206 DEG C), it can be said that 0.4TM is good approximation.Separately On the one hand, it the inventors discovered that, in the case of the silver particles sintered body of the present invention, is also shown in room temperature 298K (25 DEG C) compacted Change behavior.
The true stress-true strain curve of the silver particles sintered body of the embodiment of the present invention 1 is shown in FIG. 1.In addition, The creep behaviour (time dependent behavior of trus stress) of the silver particles sintered body of the embodiment of the present invention 1 is shown in Fig. 2.For Fig. 2 In for the creep behaviour that shows, it may be said that shown under the arbitrary measuring temperature of 298K~425K (25 DEG C~152 DEG C) according to Rely the deformational behavior (creep behaviour) in the time.That is, it can be said that the mechanical characteristic of the silver particles sintered body of the present invention and block silver (elastic-plastic behavior) difference is big, is with the silver particles sintered body with the same mechanical characteristic of resin (viscoelasticity property).Therefore, If using the silver particles sintered body of the present invention, electrical conductivity and the excellent such metalline of heat conductivity are shown, and The structure of the mechanical characteristic with resinousness can be further formed.Therefore, silver particles sintered body of the invention is used as and is used for The engagement member for engaging the component of semiconductor device is used, and can suitably be used.
The creep activity energy of the silver particles sintered body of the present invention is the 0.4~0.75 of the lattice diffusion activation energy of block silver Times.
" creep activity energy " is to refer to the silver that the Arrhenius curves of the relationship from steady state creep speed and stress acquire The apparent activation energy of microparticles sinter body." creep activity energy " in the case of block silver, corresponding to lattice diffusion activation energy.As above Described, silver particles sintered body of the invention shows creep behaviour as mechanical behavior, therefore is sintered in the silver particles of the present invention In the case of body, " creep activity energy " this term is used.
The creep activity energy of the silver particles sintered body of the present invention is less than 0.4 times of the lattice diffusion activation energy of block silver When, as engaging the engagement member of the component of semiconductor device, it is impossible to obtain sufficient sintered body intensity.In addition, this When the creep activity energy of the silver particles sintered body of invention is 0.75 times or more of the lattice diffusion activation energy of block silver, it may be said that no It can obtain sufficient creep behaviour.Therefore, in order to the silver particles sintered body of the present invention is made to be used as engaging semiconductor device The engagement member of component play defined effect, creep activity energy for the lattice diffusion activation energy of block silver 0.4~0.75 Times, preferably 0.4~0.7 times, more preferably 0.5~0.7 times, further preferably 0.53~0.63 times.Due to block silver Lattice diffusion activation energy is 190KJ/mol, therefore creep activity energy is 76~142.5KJ/mol, preferably 76~133KJ/ Mol, more preferably 95~133KJ/mol, further preferably 100.7~119.7KJ/mol.
The silver particles sintered body of the present invention preferably by the average grain diameter of primary particle is 40~350nm, crystallite grain size is 20 ~70nm and average grain diameter are heated to 130~320 DEG C of temperature and are burnt relative to the ratio between crystallite grain size for 1~5 silver particles Knot.The silver particles of the raw material for the silver particles sintered body that can be used as the present invention are illustrated.
The silver particles that can be used as the raw material of the silver particles sintered body of the present invention are characterized in that (a) primary particle is put down Equal grain size is 40~350nm, (b) crystallite grain size is 20~70nm and (c) average grain diameter relative to the ratio between crystallite grain size is 1~5.
In the present specification, average grain diameter is based on number benchmark using laser diffraction and scattering formula particle size distribution Average grain diameter.In addition, in the present specification, crystallite grain size is by utilizing the powder method of X-ray diffraction using the K α lines of Cu as line source Measure, acquire the half-peak breadth in facial index (1,1,1) face, and pass through Scherrer (Scherrer) formula calculating result.
For the silver particles that can be used as the raw material of silver particles sintered body of the present invention, the average grain diameter of primary particle For 40~350nm, preferably 40~100nm, more preferably 50~80nm.It should be noted that it can be used as the silver of the present invention The silver particles of the raw material of microparticles sinter body are usually approximate sphericity.If its average grain diameter is the range, the cohesion quilt of silver particles Inhibit, carry out being easy to get storage stability during conductive paste, be suitable as obtaining engaging semiconductor device The raw material of the engagement member of component.
For the silver particles that can be used as the raw material of silver particles sintered body of the present invention, crystallite grain size for 20~ 70nm, preferably 20~50nm.If crystallite grain size is the range, volume contraction when being burnt into is suppressed, and shape after firing Into compactness, the surface smoothness of silverskin ensured.Therefore, above-mentioned silver particles are suitable as obtaining engaging The raw material of the engagement member (silver particles sintered body of the invention) of the component of semiconductor device.
For the silver particles that can be used as the raw material of silver particles sintered body of the present invention, the average grain of a silver particles Diameter is 1~5, preferably 1~4 relative to the ratio between crystallite grain size (average grain diameter/crystallite grain size), more preferably 1~3 range. It should be noted that further preferably the lower limit of the ratio between average grain diameter is 1.5.If above-mentioned ratio is the range, it is suitable as The raw material of the conductive paste of sufficient electric conductivity is shown under firing temperature below 200 DEG C.
Can be used as the silver particles of the raw material of the silver particles sintered body of the present invention can manufacture by the following method：By carboxylic acid Silver salt and Armeen mixing, then add reducing agent, silver particles be precipitated at 20~80 DEG C of reaction temperature.
First, the silver salt of carboxylic acid and Armeen are mixed, obtains the solution for dissolving the silver salt of carboxylic acid.In solution In, it is believed that the silver salt of Armeen and carboxylic acid is coordinated, and forms a kind of amine complex.
The silver salt of carboxylic acid can be aliphatic, aromatic series any one carboxylic acid silver salt.Furthermore it is possible to it is the silver of monocarboxylic acid The polycarboxylic silver salt such as salt or dicarboxylic acids.The silver salt of aliphatic carboxylic acid can be the silver salt of chain fatty race carboxylic acid, It can be the silver salt of annular aliphatic carboxylic acid.The preferably silver salt of chain fatty race monocarboxylic acid, more preferably silver acetate, silver propionate Or butyric acid silver, particularly silver acetate.These may be used singly or in combination of two or more kinds.
Armeen can be chain fatty race primary amine or annular aliphatic primary amine.Furthermore it is possible to it is monoamine The polyamine compounds such as compound or diamine compound.Also comprising aliphatic alkyl by hydroxyl, first in Armeen The Armeen of the alkoxy substitution of oxygroup, ethyoxyl, propyl etc..More preferably 3 methoxypropyl amine, 3- aminopropanols With 1,2- diaminocyclohexanes.These may be used singly or in combination of two or more kinds.
The usage amount of Armeen depends on technologic requirement, the devices such as the post processing of silver particles of generation.From To from the perspective of the controlled silver particles of grain size, the usage amount of Armeen relative to carboxylic acid 1 equivalent of silver salt, preferably It is more than 1 equivalent.If considering influence of the superfluous Armeen to environment etc., the usage amount of Armeen is relative to carboxylic acid 1 equivalent of silver salt, preferably 1.0~3.0 equivalents, more preferably 1.0~1.5 equivalents, particularly preferably 1.0~1.1 equivalents.It is special Be not in subsequent process, by reducing agent make silver particles be precipitated liquid directly as conductive paste in use, in the presence of The possibility that surplus Armeen is gasified by heating.It is therefore especially preferred that using the above-mentioned range it is preferable to use amount.
The mixing of the silver salt and Armeen of carboxylic acid can be in the state of there is no organic solvent or there are organic molten It is carried out in the state of agent.By using organic solvent, mixing can be made easy.As organic solvent, ethyl alcohol, third can be enumerated The alcohols such as alcohol, butanol；The ethers such as propylene glycol dibutyl ethers；And aromatic hydrocarbons such as toluene etc..These can be used alone or simultaneously Use two or more.The viewpoint of the usage amount of organic solvent from the productivity of the silver particles in the convenience of mixing, subsequent process goes out Hair, can the amount of being arbitrary.
The mixing of the silver salt and Armeen of carboxylate for example, by side stir Armeen or Armeen with The silver salt of carboxylic acid is added to carry out in the mixture of organic solvent, side.It can also suitably continue to stir after addition.In this phase Between, preferably keep the temperature at 20~80 DEG C, more preferably 20~60 DEG C.
Then addition reducing agent, is precipitated silver particles.As reducing agent, from the viewpoint of being reacted control, preferably formic acid, Formaldehyde, ascorbic acid or hydrazine, more preferably formic acid.These may be used singly or in combination of two or more kinds.
The usage amount of reducing agent be usually for the oxid-reduction equivalent of the silver salt of carboxylic acid more than, oxid-reduction equivalent is preferred It is 0.5~5 times, more preferably 1~3 times.The silver salt of carboxylic acid is the silver salt of monocarboxylic acid, when using formic acid as reducing agent, formic acid By mole usage amount of conversion relative to 1 mole of the silver salt of carboxylic acid, preferably 0.5~1.5 mole, more preferably 0.5~1.0 rubs You, further preferably 0.5~0.75 mole.
In addition reducing agent and subsequent reaction, 20 DEG C~80 DEG C are kept the temperature at.Temperature is preferably 20~70 DEG C, More preferably 20~60 DEG C.If temperature is within that range, the grain growth of silver particles is abundant, and productivity is also high, in addition two Secondary cohesion is also inhibited.Reducing agent and subsequent the desired Time Dependent of reaction are added in the Regulations moulds of reaction unit, usually 10 minutes~10 hours.It should be noted that when adding reducing agent and subsequent reaction, it can be as needed, with additional Form addition is selected from the aromatic hydrocarbons such as ethers and toluene such as alcohols, the propylene glycol dibutyl ethers such as ethyl alcohol, propyl alcohol and butanol etc. Organic solvent.
In addition reducing agent and subsequent reaction, the amount (mol) of the silver salt of carboxylic acid is relative to by the silver salt and fat of carboxylic acid Total volume (L) of the mixed solution of fat race primary amine, reducing agent and arbitrary organic solvent preferably become 1.0~ The range of 6.0mol/L, more preferably 2.0~5.0mol/L, further preferably 2.0~4.0mol/L.If the silver salt of carboxylic acid Concentration within that range, then fully can carry out the stirring of reaction solution and remove reaction heat, therefore the silver particles being precipitated is flat Equal grain size becomes appropriate.And then obstacle will not be brought to the operations such as the sedimentation decantation in subsequent handling and solvent displacement.
It is put into reaction vessel by the silver salt of carboxylic acid and the mixed solution of Armeen and arbitrary organic solvent, When being reacted with the semi-batch mode for continuously feeding reducing agent, the silver salt and the mixed solution of Armeen of carboxylic acid, Total volume of reducing agent and arbitrary organic solvent is every from the required time for starting to add reducing agent to reaction end per 1L The amount of precipitation of the silver particles of 1 hour can be set as the range of 0.3~1.0mol/h/L, therefore productivity is very big.With continous way Reactive mode (continous way is thoroughly mixed grain, flow type) implements that during reaction higher productivity can be obtained, and industrialness is implemented Give very golden eggs.
The narrow particle size distribution of the silver particles obtained in this manner, it is less than 2.0 that can make geometric standard deviation.At this In specification, geometric standard deviation is 84.3% grain size of the number benchmark based on laser diffraction and scattering formula particle size distribution The ratio between (D84.3 values) and 50% grain size (D50 values) (D84.3 values/D50 values).
It can make the removing supernatant such as decantation is settled and passed through by the silver particles that reaction is precipitated or first can be added The alcohol such as alcohol, ethyl alcohol or terpinol equal solvent simultaneously point take.Layer containing silver particles can be used directly as conductive paste.It is conductive Silver-containing rate in the preferred conductive paste of paste is 40~90 weight %, more preferably 45~80 weight %.
The silver particles sintered body of the present invention can by by above-mentioned silver particles by being detached from solvent, and at the specified temperature It is sintered and obtains.But from the easiness grade of operation, it will preferably contain in the conventionally known method such as silk screen print method The conductive paste for having above-mentioned silver particles prints or after being coated on the part of requirement of base material etc., by be heated to set point of temperature come It is sintered, so as to obtain the silver particles sintered body of the present invention.Furthermore it is also possible in the conductive paste containing above-mentioned silver particles Middle hybrid resin, the curable resin such as epoxy resin are sintered by being heated to set point of temperature, so as to be contained The silver particles sintered body of resin.In the case, the gap of silver particles sintered body is filled by resin.The silver particles sintering of the present invention Even if body when containing resin, the curable resin such as epoxy resin, can also show very high electric conductivity, and table Reveal special creep behaviour.
Can be used as the raw material of the silver particles sintered body of the present invention containing silver particles or silver particles it is conductive paste, in order to The heating temperature being sintered is 130~320 DEG C, preferably 140~320 DEG C, more preferably 150~300 DEG C, further preferably It is 150~200 DEG C.In addition, in order to which the lower limit for the heating temperature being sintered is particularly preferably 130 DEG C, the upper limit is particularly preferably 250℃.The silver particles sintered body as obtained from being burnt under the heating temperature shows very high electric conductivity (example Such as, 1~10 μ Ω cm of specific resistance value are horizontal), and show special creep behaviour.
It can be used as the heating of the conductive paste containing silver particles or silver particles of the raw material of the silver particles sintered body of the present invention Time is according to heating temperature and different.In general, heating time can be the range of 5 minutes~60 minutes, preferably 10 minutes~ The range of 30 minutes.As an example, it is heated at a temperature of 200 DEG C in an atmosphere and is sintered the conductive paste containing silver particles When, by being set as the heating time of 15 minutes or so, the silver particles with special creep behaviour and high conductivity can be obtained Sintered body.
It can be used as the heating of the conductive paste containing silver particles or silver particles of the raw material of the silver particles sintered body of the present invention (firing) can carry out in an atmosphere.Must make in the case of conductive paste solvent volatilize and/or burning, therefore preferably containing In oxygen atmosphere, for example heated in oxygen atmosphere or air.As device for heating, well known electric furnace etc. can be used Firing furnace.
The silver particles sintered body of the present invention can be using the silver particles obtained in the manner described above as primary particle, by pressing It is sintered and obtains according to aforesaid way.That is, the manufacturing method of the silver particles sintered body of the present invention includes following process：It will be primary The average grain diameter of particle is 40~350nm, crystallite grain size is 20~70nm and average grain diameter relative to the ratio between crystallite grain size be 1~ The process that 5 silver particles are sintered at 120~300 DEG C of temperature.It is used by regarding above-mentioned silver particles as primary particle Manufacture silver particles sintered body, can effectively obtain can mitigating semiconductor device stress and it is conductive, use In the engagement member of the component of engagement semiconductor device.
The present invention relates to the semiconductor device that semiconductor chip is engaged with supporting mass by engagement member, and it is engagement member Semiconductor device for above-mentioned silver particles sintered body.If the silver particles sintered body of the present invention is used as to engage semiconductor chip With the engagement member (die bonding material) of supporting mass, then since exothermic character is very excellent, can efficiency spread well by half The heat that conductor element generates.In addition, the silver particles sintered body of the present invention can be used as to replace the high thermal conductivity chip of kupper solder It is bonded material.
It is partly led via what convex block engaged with wiring substrate or the second semiconductor chip the present invention relates to the first semiconductor chip Body device, and be convex block part or all be above-mentioned silver particles sintered body semiconductor device.The silver particles of the present invention Sintered body may be used as the convex block of semiconductor device.Particularly preferably the silver particles sintered body of the present invention is used as partly leading for engaging Convex block of the body chip with wiring substrate or for engaging two semiconductor chips (the first and second semiconductor chips).In addition, it is Engagement has the semiconductor chip of copper pillar bumps, and a part that silver particles sintered body of the invention is also used as convex block makes With.In addition, when semiconductor device has the following structure, i.e., three or more semiconductor chips, silicon intermediary layer exist across grafting material When many places are mutually coupled respectively, the silver particles sintered body of the present invention can be used as the grafting material in many places for engagement. If the silver particles sintered body for the present invention for showing creep behaviour to be used as to the convex block of semiconductor device, even if being generated in convex block During stress, it is also possible to prevent bad in convex block generation crackle etc..Even if the stress generated to semiconductor device becomes larger, also can Prevent the breakage of semiconductor device.In addition, since the silver particles sintered body of the present invention is using silver as material, it can also be suitable Ground is used as the convex block of the big flip-chip semiconductor device of calorific value.It in addition, can also when for current density big convex block Inhibit electromigration.In addition, the silver particles sintered body of the present invention is easily formed, the manufacture of semiconductor device is accordingly used in, can be obtained To high productivity.
The present invention relates to the manufacturing methods of semiconductor device that semiconductor chip is engaged with supporting mass by engagement member.
The manufacturing method of the semiconductor device of the present invention includes following process：It is 40 by the average grain diameter containing primary particle The conductive paste confession of~350nm, the silver particles that crystallite grain size is 20~70nm and the ratio between average grain diameter and crystallite grain size are 1~5 To the process on supporting mass.The supporting masses such as the substrate used in semiconductor element are well known.It is supplied as by conductive paste Method on to supporting mass can enumerate silk screen print method etc..As for engaging the engagement member of the component of semiconductor device, If silver particles as defined in above-mentioned are used as raw material, exothermic character is very excellent, thus can efficiency spread well by The heat that the component of semiconductor element generates.
The manufacturing method of the semiconductor device of the present invention is included in semiconductor chip alignment position mounting on supporting mass Process.Position alignment and placement for semiconductor chip can use well known method.
The manufacturing method of the semiconductor device of the present invention includes：Supporting mass, conductive paste and semiconductor chip are heated to 120~300 DEG C of temperature and carry out process.By heating conductive paste in defined temperature, can will show defined compacted The silver particles sintered body of the present invention of change behavior is configured as the engagement member of supporting mass and semiconductor chip.If use this hair The manufacturing method of bright semiconductor device can then mitigate the stress of the engagement on supporting mass between semiconductor chip, therefore It can inhibit to result from crackle of semiconductor device etc..
The present invention relates to the manufacturing methods of the semiconductor device with convex block.
The manufacturing method of the semiconductor device with convex block of the present invention includes, and is by the average grain diameter containing primary particle The conductive paste of 40~350nm, the silver particles that crystallite grain size is 20~70nm and the ratio between average grain diameter and crystallite grain size are 1~5 It supplies to the process of semiconductor chip.It is supplied as by conductive paste to the method for semiconductor chip, silk-screen printing can be enumerated Method etc..
The manufacturing method of the semiconductor device with convex block of the present invention includes：Semiconductor chip is heated to temperature 120 ~300 DEG C and carry out process.By heating conductive paste in defined temperature, defined creep behaviour can will be shown The silver particles sintered body of the present invention is configured as the convex block of semiconductor device.If this hair of creep behaviour as defined in showing Bright silver particles sintered body is used as the convex block of semiconductor device, even if being then also possible to prevent when convex block generates stress in convex block It is bad that crackle etc. occurs.In addition, when the stress generated to the semiconductor device obtained by the manufacturing method of the present invention becomes larger, It can prevent the breakage of semiconductor device.
Embodiment
The silver particles sintered body of the trial-production present invention in the following order.That is, making the conductive paste containing silver particles first, connect It and the conductive paste is printed on glass slide and is burnt into.
The manufacturing method of the conductive paste containing silver particles of Examples 1 to 3 and comparative example 1 and 2 is as follows.10L's 3 methoxypropyl amine 3.0kg (30.9mol) is added in glass system reaction vessel.Reaction temperature is maintained at 45 DEG C while stirring Hereinafter, and add silver acetate 5.0kg (30.0mol).Just addition after become transparent solution and dissolve, but with addition into Row, solution is gradually muddy, if addition whole amount, becomes the viscous solution of grey tea dull colour.95 weight % are slowly added dropwise thereto Formic acid 1.0kg (21.0mol).Fierce heat release can be confirmed after being just added dropwise, during this period, reaction temperature is maintained at 30 ~45 DEG C.Originally, the viscous solution of grey dull colour becomes black by dark brown.Terminate reaction after whole amount is added dropwise.Reaction is mixed Object is divided into two layers when standing for 40 DEG C.Upper strata is the transparency liquid of yellow, and the silver particles of black are settled out in lower floor.The liquid on upper strata Not argentiferous ingredient in body.The liquid on upper strata is removed by decantation, layer separation is carried out using methanol and obtains 65 weight % of silver-containing rate Conductive paste.
The average grain diameter of silver particles contained in obtained conductive paste and crystallite grain size are measured, as a result average grain diameter is 100nm, crystallite grain size are 40nm.The average grain diameter of silver particles is 2.5 relative to the ratio between crystallite grain size as a result,.
The conductive paste obtained in the manner described above is printed in a manner of becoming mechanical test plate shape shown in fig. 5 On glass slide, it is burnt by heating.Heating condition is as shown in table 1.That is, in the case of example 1, at 353K (80 DEG C) After being kept for 30 minutes, heated 30 minutes under the heating temperature of 423K (150 DEG C).Silver particles are sintered by the heating, can be with Obtain the silver particles sintered body of embodiment 1.Equally, in the case of embodiment 2 and 3 and comparative example 1 and 2, in 353K (80 DEG C) keep 30 minutes after, heated 30 minutes under the defined heating temperature shown in table 1.
Obtained Examples 1 to 3 and the resistivity and thermal conductivity of the sample of comparative example 1 and 2 are measured.It is tied Fruit is shown in Table 1.Thermal conductivity utilizes Measurement By Laser Flash.It should be noted that in the silver particles sintered body of comparative example 1 In the case of, the curing film-strength of silver particles sintered body is low, therefore cannot measure activation energy.In addition, in the silver particles of comparative example 2 In the case of sintered body, sintering shrinkage is big and crackle occurs in the cured film of silver particles sintered body, therefore cannot measure activation Energy.
[table 1]
The mechanical characteristic of the silver particles sintered body of embodiment 1 is determined.Specifically, it has carried out determining rate of straining Tensile test and stress mitigate experiment.Mechanics machine uses the micro mechanics testing machine that piezoelectric element is employed to actuator.It is anti- Drawing experiment is 10 according to rate of straining- 1/ second (/sec), 10- 2/ the second and 10- 3This 3 levels of/second, test temperature 298K, 328K, 358K, 388K and 423K this 5 levels carry out.In stress mitigates experiment, apply elongation strain to norminal strain Until 0.3~2.1%, strain 1000 seconds is then kept.
Trus stress (longitudinal axis, the MPa)-true strain (horizontal axis, %) that the silver particles sintered body of embodiment 1 is shown in FIG. 1 is bent Line.In addition, the stress that the silver particles sintered body of embodiment 1 is shown in FIG. 2 mitigates result of the test.In fig. 2, with the time (second) For horizontal axis, represented with trus stress (MPa) for the longitudinal axis.It is 10 in Fig. 1 and the rate of straining of tensile test shown in Fig. 2- 3/ the second. Result can clearly be learnt as shown in Figure 1, and as the temperature increases, spring rate and stress reduce the silver particles sintered body of embodiment 1, There is viscous behavior.In addition, as shown in Fig. 2, the silver particles sintered body of embodiment 1 is in the entire survey from room temperature (298K) to 423K Stress peaceable conduct is observed in the range of constant temperature degree.I.e., it is known that the silver particles sintered body of embodiment 1 is different from block silver, performance Go out to be similar to the mechanical behavior of resin material.According to the above, it may be said that the silver particles sintered body of embodiment 1 is at least in block The temperature of the creep start temperature (206 DEG C) of silver below starts creep.In ag material, such mechanics is not shown in the past The report example of behavior.Thus, it is possible to the silver particles sintered body for saying the present invention is show extremely interesting mechanical behavior novel Ag material.
The steady state creep speed of silver particles sintered body of embodiment 1 and the relationship of stress is shown in FIG. 3.In addition, Fig. 4 pairs Arrhenius curves are shown in the steady state creep speed of embodiment illustrated in fig. 31 and the relationship of stress.According to based on The parsing of Arrhenius curves, the apparent activation energy (creep activity energy) for calculating the silver particles sintered body of embodiment 1 are 105KJ/ mol.The value is 0.55 times of the lattice diffusion activation energy (190KJ/mol) of block silver.
Similarly to Example 1, according to the parsing based on Arrhenius curves, the silver of embodiment 2 and embodiment 3 is obtained The apparent activation energy (creep activity energy) of microparticles sinter body, the activation energy of acetonideexample 2 are 118KJ/mol, the work of embodiment 3 Change can be 131KJ/mol.These values be the lattice diffusion activation energy (190KJ/mol) of block silver 0.62 times (embodiment 2) and 0.69 times (embodiment 3).
According to result above it may be speculated that the silver particles sintered body of Examples 1 to 3 is different from the lattice diffusion of block silver, Creep is spread by grain circle come rate controlling.It can speculate：The silver particles sintered body of the present invention has the knot that grain circle structure is easily spread Structure, therefore visible creep behaviour.It is possible thereby to clearly, silver particles sintered body of the invention has electrical characteristics and heat-transfer character for gold Attribute but shows this extremely special property of the mechanical characteristic of resinousness.
It should be noted that as described above, in the case of the silver particles sintered body of comparative example 1 and comparative example 2, occur low Curing film-strength and the problem of cracking, therefore activation energy cannot be measured.It specifies, is 393K (120 in heating temperature DEG C) below in the case of, occur silver particles sintered body this low problem of curing film-strength.In addition it specifies, in heating temperature In the case of for more than 623K (350 DEG C), this problem that cracks is happened in the cured film of silver particles sintered body.
In addition, following parsing is carried out to the silver particles sintered body of the present invention.
For the mechanical behavior of the silver particles sintered body of the clear and definite present invention, Finite Element parsing (FEM) has been carried out.Scheming The internal structure (2 charge patterns) of the silver particles sintered body of the present invention is shown in 6.It is deposited inside the silver particles sintered body of the present invention In a large amount of hole.Therefore, the mechanical characteristic of sintered test film is the apparent characteristic of the material containing a large amount of holes, not Only show the mechanical characteristic of silver-colored sintering portion (compact part).In order to study the deformation mechanism for being related to the silver particles sintered body of the present invention Details, it is necessary to study the deformation mechanism of the compact part.Therefore in this parsing, the silver particles that the present invention is reproduced with FEM model are burnt Microstructure inside knot body against analyticity acquires the characteristic of silver-colored compact part in a manner of meeting apparent mechanical behavior. The FEM analytic modell analytical models of the silver particles sintered body of the present invention are shown in Fig. 7.Use FIB (Focused Ion Beam：Focused ion Beam) the silver particles sintered body of the present invention is cut off with 15nm intervals, the profile image of acquirement is made to be imaged and form the micro- of 1 μm of square See Scale Model.Cell type ties up unit, number of nodes about 250,000 for 4 face bodies 2.Analysis software uses ANSYS ver.13, this hair Bright silver particles sintered body follows elastic-plastic-creep behavior, by steady state creep structure shown in the approximate hardening rule of 2 straight lines and (1) formula An accepted way of doing sth combines to implement to parse.
Here, εssFor steady state creep rate of straining, A is material constant, and σ is stress, and n is stress exponent.Spring rate and plus Work curing characteristics is acquired by the result obtained by determining rate of straining tensile test, in addition, creep properties use is mitigated by stress The result that experiment obtains against analyticity acquires.
Tensile test result (solid line) is shown in FIG. 8, in addition, representing that stress mitigates result of the test (solid line) in fig.9. First, from the point of view of tensile test result, silver particles sintered body of the invention shows linear behavior near room temperature, in true strain 0.5% nearby becomes the brittle behaviour of fracture.In addition, the stress reduction with temperature rise of the silver particles sintered body of the present invention, And as non-linear behavior.Become the stress behavior of dynamic recovery type if more than 388K, signal becomes the deformation of creep.Separately Outside, it is conceived to spring rate, is understood by experimental result at room temperature for 12.4GPa, the pole compared with the Young's modulus 76GPa of block silver It is low.The porosity of the silver particles sintered body of the present invention is 30% or so, considers to be also extremely low value in this respect.The result is illustrated： The mutual bonding of silver particles is weaker than block silver.
Then, the stress peaceable conduct of the silver particles sintered body of the present invention is observed, has obtained interesting result：From common The room temperatures of the 0.4TM (with 40% temperature of Kelvinometer fusing point) of the empirical rule of creep performance below are observed slow With.If considering, Young's modulus is low and creep occurs even if at low temperature, it is envisioned that the bonded interface of silver particles is formed Special structure.
In order to study such special deformation mechanism, using microstructure FEM model shown in Fig. 7 as elastic-plastic-creep Body, the result that the characteristic of the compact part of silver is carried out to inverse parsing are shown in white hollow mark in Fig. 8 and Fig. 9.It will acquire at this time Silver compact part creep properties it is shown in Figure 10.The stress exponent n of slope as figure takes 4~8 value at each temperature, Thus it is shown that stress exponent as dislocation creep.The result is acquired into constitutional formula using hyperbola approximation, is (2) formula.
Here, rate of straining, stress, temperature and activation energy unit be respectively s- 1(/ the second), MPa, K and J/mol.Creep It is 105kJ/mol that activation energy, which uses the result of the best match of (2) formula, is the lattice diffusion activation energy (190kJ/ of block silver Mol) approximately half of.From the viewpoint of diffusion, it is believed that not dislocation creep caused by lattice diffusion, and grain circle is spread It is the rate controlling mechanism of creep.If in this regard, consider together foregoing Young's modulus than block silver it is low the fact, it may be considered that Even if mutual engagement grain circle of silver particles has the thick structure of the comparison for being also easy to diffusion at low temperature.The silver particles of the present invention are burnt Knot body has such thick grain circle structure, this is considered related with the special mechanical behavior for embodying creep at low temperature.
By these results it can be said that can expect using the silver particles sintered body of the present invention as compared with can also delay under low temperature With the materials with high melting point of stress.
In above-mentioned parsing, the result for carefully studying the low-temperature creep behavior of the silver particles sintered body of the present invention specifies The following contents.
(1) silver particles sintered body of the invention shows brittle behaviour at low temperature, and dynamic is showed with the rising of temperature The stress behavior of reply type.In addition, Young's modulus is low compared to block galactic pole, consider that porosity is also extremely low value, therefore can To think that the mutual bonding of silver particles is weaker than block silver.
(2) silver particles sintered body of the invention known to is from the room of below the 0.4TM of empirical rule that common creep shows Temperature, which rises, occurs stress mitigation, shows creep at low temperature.
(3) for the creep of the present invention, it is believed that the diffusion of grain circle is rate controlling mechanism, if considering Young mould together The fact that amount is lower than block silver, even if it is thick with the comparison for being also easy to diffusion at low temperature then to envision mutual grain circle of silver particles Grain circle structure.
(embodiment 4)
Then, epoxy resin and the firing as curable resin are further mixed into the conductive paste of embodiment 1, is removed Other than this, the silver particles sintered body of embodiment 4 is made similarly to Example 1.The silver particles sintered body of embodiment 4 includes curing Property resin.Epoxy resin has used hexahydrophthalic acid 2-glycidyl ester.In addition, relative to 100 parts by weight of silver particles, ring The additive amount of oxygen resin is 3.5 parts by weight.
The stress that the silver particles sintered body comprising curable resin of embodiment 4 is shown in FIG. 11 mitigates result of the test. It should be noted that in order to be compared, the stress for also showing the silver particles sintered body of embodiment 1 in fig. 11 mitigates experiment As a result.Can be clear and definite by Figure 11, for the silver particles sintered body comprising curable resin of embodiment 4, observe and real Apply the same stress peaceable conduct of silver particles sintered body of example 1.It can be clear and definite：The silver particles sintered body of embodiment 4 and block silver Difference shows the mechanical behavior similar to resin material.

Claims (8)

1. a kind of silver particles sintered body is for engaging the sintering of the die bonding timber-used silver particles of the component of semiconductor device Body,
Wherein, the creep activity energy of silver particles sintered body is 0.4~0.75 times of the lattice diffusion activation energy of block silver.
2. silver particles sintered body according to claim 1, wherein, silver particles sintered body is micro- to the silver as primary particle The sintered body that grain is sintered,
The average grain diameter of primary particle is 40~350nm, crystallite grain size is 20~70nm and average grain diameter is relative to crystallite grain size The ratio between be 1~5.
3. silver particles sintered body according to claim 1 or 2, wherein, the creep activity energy of silver particles sintered body is block 0.4~0.7 times of the lattice diffusion activation energy of silver.
4. silver particles sintered body according to claim 1 or 2 is by the way that the silver particles of primary particle are heated to temperature 130~320 DEG C are sintered.
5. silver particles sintered body according to claim 1 or 2, wherein, the gap of silver particles sintered body is filled by resin.
6. a kind of semiconductor device is the semiconductor device that semiconductor chip is engaged with supporting mass by die bonding material, wherein, Die bonding material is the silver particles sintered body described in any one of Claims 1 to 5.
7. a kind of manufacturing method of silver particles sintered body is for engaging the die bonding timber-used of the component of semiconductor device silver The manufacturing method of microparticles sinter body,
Including：By be 40~350nm by the average grain diameter of primary particle, crystallite grain size is 20~70nm and average grain diameter is opposite In the silver particles that the ratio between crystallite grain size is 1~5 after 80 DEG C are dry, the work that is heated to 130~320 DEG C of temperature to be sintered Sequence,
The creep activity energy of silver particles sintered body is 0.4~0.75 times of the lattice diffusion activation energy of block silver.
8. a kind of manufacturing method of semiconductor device is the semiconductor that semiconductor chip is engaged with supporting mass by die bonding material The manufacturing method of device,
Including：By the average grain diameter comprising primary particle be 40~350nm, crystallite grain size is 20~70nm and average grain diameter is opposite The process to supporting mass is supplied in the conductive paste for the silver particles that the ratio between crystallite grain size is 1~5；
By the process of semiconductor chip alignment position mounting on supporting mass；With
By by supporting mass, conductive paste and semiconductor chip at 80 DEG C it is dry after, be heated to 130~320 DEG C of temperature to carry out The process of sintering, the creep activity energy of silver particles sintered body are 0.4~0.75 times of the lattice diffusion activation energy of block silver.
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